SU1060108A3 - Process for preparing cyanur chloride having high reactivity in aqueous solution or suspension - Google Patents

Abstract

Process for the production of cyanuric chloride mixtures in which the cyanuric chloride is resistant to agglomeration during storage and handling and is resistant to undesirable hydrolysis, without reducing the reactivity of the cyanuric chloride with respect to organic reactants. The present mixtures contain cyanuric chloride and a minor amount by weight of a finely divided, inert, hydrophobic filler material to form a new, homogeneous, particulate cyanuric chloride composition in which the cyanuric chloride particles are surrounded by the inert filler particles.

Description

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The invention relates to methods for producing cyanuric chloride, which is highly reactive in an aqueous solution or suspension, of an initial product in the synthesis of herbicides, optical brighteners and vulcanizing agents. When carrying out the process with the use of highly cooled aqueous solutions or suspensions, rapid passage is necessary. Otherwise the hydrolysis takes place to a significant degree with the formation of cyanuric acid. On the day of acceleration of the process, the solution or suspension of cyanuric chloride in water is subjected to mechanical grinding of C1. The disadvantages of this method are the high corrosivity of the process associated with the formation of hydrogen chloride in the process of hydrolysis, and the possibility of contamination of the target product with CORROSION products. Closest to the proposed method for producing cyanuric chloride, which has a high reactivity, is that liquid molten cyanuric chloride t "146 C) is blown into the appropriate solvent, which results in rapid cooling to obtain sufficiently small particles 112. The disadvantages of this method are the complexity of the work (transport storage and introduction of cyanuric chloride into liquid CIM at temperatures; c) 1–146 ° С, high energy consumption and process corrosion. The purpose of the invention is to simplify the method of producing highly reactive cyanuric chloride in an aqueous solution or suspension. The goal is achieved by the fact that according to the proposed method / into the gaseous stream of cyanuric chloride, the volume of the hydrophobic filler with a degree of dispersion of 10-20. The hydrophobic catalyst is introduced into the gaseous stream before or after sublimation. In cyanuric chloride, small particles of cyanurine are surrounded by a hydrophobic substance and counteract undesirable hydrolysis and at the same time do not interfere with the reaction with organic components. In addition, the formed cyanuric chloride particles are protected from secondary agglomeration. Therefore, cyanuric chloride also has flowing properties. As fillers, cyanuric chloride can contain all substances that do not react with cyanuric chloride, i.e. are inert with respect to cyanuric chloride and its reaction partners and products. It should be borne in mind both inorganic and organic fillers. Hydrophobic properties may be intrinsic to fillers, however they may be imparted by appropriate treatment, for example, silanes and similar compounds. Hydrophobic pyrogenic or precipitated silicic acid, alumina, aluminum silicates, calcium silicate and mixtures thereof are commonly used. The hydrophobic filler is used in an amount of 0.1–3 wt.% (Especially 0.2–0.7 May. Vi, considering the total mixture. The preparation of cyanuric chloride is carried out by intensive mixing with cyanuric chloride gas before desublimation or immediately after desublimation. Example 1 , In the gas stream, consisting of 200 kg / h of cyanuric chloride vapor and 150 kg / h of air, which is fed into the condenser, immediately before being introduced into the condenser, 1.0 kg / h of hydrophobic pyric silicic acid with a particle size of 12 pm are mixed. additionally for homogenization mechanical mixing in the mixer still exists. If cyanuric chloride thus obtained is used in the synthesis of atrazine in an aqueous solution or suspension, the content of atrazine is 96% or more. If atrazine is synthesized in the same way with cyanuric chloride without adding hydrophobic silicic acid and without mechanical grinding, an atrazine content of 90-92% is obtained. EXAMPLE 2 According to Example 1, 200 kg / h of cyanuric chloride vapor and ISO kg / h of air introduced into the condenser at the gas stream are added directly Before entering into the condenser О, 2 kg / h of hydrophobic pyrrhenic silicic acid with the size of Chartz - “12 pm. With the change of the scientific research institute of the aggregative state of cyanur chloride from vapor to solid, a process similar to Example 1 takes place. Example 3. In a gas stream of 200 kg / h of a pair of cyanuric chloride and 150 kg / h of air introduced into a condenser at 180 ° C, immediately before entering into the condenser 20 kg / h of hydrophobic pyrogenic silicic acid with a particle size of pm. When the aggregate state of chloride cyanur changes from vapor to solid state, the process proceeds as in example 1.

Example 4. A 200 kg / h of cyanur chloride vapor and 150 kg / h of air introduced into a condenser at 18 ° C are added to the gas stream just before entering 0.4 kg / h of a hydrophobic pyrogenic silicic acid with a particle size 12 pm

Example 5. To a gas stream of 200 kg / h of a pair of cyanure chloride and 150 kg / h of air introduced into the condenser at 180 s, 1.4 kg / h of hydrophobic pyrogenic silicic acid with a particle size of / 12 pm were added immediately before entering the condenser. .

Example 6. To a gas stream of 200 kg / h of a vapor of cyanur chloride and 150 kg / h of air introduced into the condenser with, just before entering into the condenser 1.0 kg / h of hydrophobic precipitated silicic acid with a particle size of 13 pm are added.

Example 7. A 200 kg / h of cyanur chloride vapor and 150 kg / h of air introduced into the -v capacitor at 180 ° C are added to the gas stream immediately before entering the condenser with a particle size of 20 kg / h of a hydrophobic alumina. pm

Example 8. In a gas stream 200 kg / h of a vapor of cyanur chloride and 150 kg / h of air introduced into a condenser at 180 ° C are added immediately before entering the condenser 1.0. Kg / h of hydrophobic aluminum silicates with a particle size of 10 -20 pm

Example 9. A 200 kg / h of cyanur chloride vapor and 150 kg / h of air introduced into a condenser at 180 ° C are added to the gas stream just before entering 1.0 kg / h of hydrophobic calcium silicate with a particle size of l-10 into the condenser. -20 pm

PRI me R 10. In the gas stream 200 kg / h of a pair of cyanure chloride and

130 kg / h of air introduced into the condenser when a mixture of 0.5 kg / h of hydrophobic pyrogenic silicic acid with a Chartz size of 12 pm and 0.5 kg / h of hydrophobic calcium silicate with a particle size is added just before entering the condenser.

| 10-20 pm

Example 11. 200 kg of freshly condensed cyanuric chloride are introduced into a mixing device and mixed in it with 1.0 kg of hydrophobic pyrogenic silicic acid with a particle size of 12 pm.

Example 12; At the gas flow, 5 consisting of 100 kg / h of cyauric chloride vapor and 75 kg / h of air, just before introduction, 0.1 kg of hydrophobic pyrogenic silicic acid with a particle size of 12 pm is added to the condenser. When cyanuric chloride is separated, cyanuric chloride particles are covered with hydrophobic silicic acid. The cyanuric chloride thus prepared in a water suspension without further processing is treated with the appropriate amine to obtain 2-ethyl-amino-4-. -chloro-6-isopropylamino-1,3,5-triazine (. atrazina. The content of atrazine in the product g of the reaction is 96.1%.

Example 13. To a gas stream of 150 kg / h of cyanuric chloride vapor and 115 kg / h of air at 180 ° C, 15 kg / h of hydrophobic pyropenic silicic acid with a particle size ("12 pm."

The cyanuric chloride thus obtained, without further processing in aqueous suspension, is treated with ethylamine and isopropyllamine to synthesize atrazine. Conversion 96.8%.

The sieve analysis of the products prepared according to examples 1-10 as compared with the sieve analysis of cyanuric chloride obtained without the addition of a hydrophobic filler is listed in ... the table.

Hydro cutting supplements

Claims (3)

1. METHOD FOR PRODUCING CYANUR-. . CHLORIDE HAVING A HIGH REACTIVITY IN AQUEOUS SOLUTION OR SUSPENSION, characterized in that, in order to simplify the process and increase the reactivity of the target product, 0.1-10 wt.% Hydrophobic filler with a dispersion degree of 10- is introduced into the gaseous stream of cyanuric chloride 20 lm 2. The method according to claim 1, about the name of u and And with that. That the filler is introduced into the gaseous stream before sublimation. 3. The method according to π.1, wherein the filler g is administered after sublimation. ® cl s> its reaction partners and reaction products. It should be borne in mind both inorganic and organic fillers. Hydrophobic properties may be inherent in fillers, however, they may be imparted as a result of appropriate treatment, for example, with silanes and similar compounds. Hydrophobic pyrogenic or precipitated silicic acid, alumina, aluminum silicates, calcium silicate and mixtures thereof are usually used. The hydrophobic filler is used in an amount of 0.1-3 wt.% (Especially 0.2-0.7 may.%), Based on the total mixture. The preparation of cyanuric chloride is carried out by intensive mixing with gaseous cyanuric chloride before desublimation or immediately after desublimation. Example 1. In a gas stream containing 200 kg / h of cyanuric vapor which is fed at 180 ° C into a condenser, immediately before introducing into the condenser, 1.0 kg / h of hydrophobic pyrogenic silicic acid with a particle size of? <12 pm are mixed. Additionally, for homogenization, mechanical mixing is also carried out in a mixer. If the cyanuric chloride thus obtained is used in the synthesis of atrazine in an aqueous solution or suspension, the content of atrazine is obtained in 96% or more. If atrazine is synthesized in the same way with cyanuric chloride without the addition of hydrophobic cream acid 40 and without mechanical grinding, then an atrazine content of 90-92% is obtained. PRI me R 2; According to example 1, in a gas stream of 200 kg / h steam of cyanuric chloride and 150 kg / h of air introduced into the condenser at 180 ° C, is added immediately before the introduction of 0.2 kg / h of hydrophobic pyrogenic silicic acid with a particle size of 50 - 12 pm When the state of aggregation of chloride changes. cyanuric from occurs measure 1.